CN104120037A - Extracting method for jasmine flower essential oil - Google Patents
Extracting method for jasmine flower essential oil Download PDFInfo
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- CN104120037A CN104120037A CN201410387956.1A CN201410387956A CN104120037A CN 104120037 A CN104120037 A CN 104120037A CN 201410387956 A CN201410387956 A CN 201410387956A CN 104120037 A CN104120037 A CN 104120037A
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- 235000010254 Jasminum officinale Nutrition 0.000 title claims abstract description 170
- 239000000341 volatile oil Substances 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 21
- 240000005385 Jasminum sambac Species 0.000 title 1
- 241000207840 Jasminum Species 0.000 claims abstract description 169
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000000284 extract Substances 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000000605 extraction Methods 0.000 claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 29
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003921 oil Substances 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 40
- 239000012141 concentrate Substances 0.000 claims description 35
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000469 ethanolic extract Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 3
- 238000007710 freezing Methods 0.000 abstract description 2
- 230000008014 freezing Effects 0.000 abstract description 2
- 239000012165 plant wax Substances 0.000 abstract description 2
- 239000013557 residual solvent Substances 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 42
- 239000003960 organic solvent Substances 0.000 description 32
- 239000004215 Carbon black (E152) Substances 0.000 description 26
- 229930195733 hydrocarbon Natural products 0.000 description 26
- 150000002430 hydrocarbons Chemical class 0.000 description 26
- 229910002092 carbon dioxide Inorganic materials 0.000 description 21
- 239000003795 chemical substances by application Substances 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 239000002253 acid Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 238000004821 distillation Methods 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 239000012178 vegetable wax Substances 0.000 description 2
- 208000032544 Cicatrix Diseases 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 206010040925 Skin striae Diseases 0.000 description 1
- 208000031439 Striae Distensae Diseases 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000003048 aphrodisiac agent Substances 0.000 description 1
- 230000002509 aphrodisiac effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000037336 dry skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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Abstract
一种茉莉花精油的提取方法，对用石油醚或正戊烷浸提制得的茉莉花浸膏，通过乙醇溶解冷冻脱除植物蜡杂质，蒸馏回收溶剂乙醇，水洗脱醇制得粗茉莉精油，将粗茉莉精油用超临界CO2进一步分离除去残留溶剂，制得香味纯正的茉莉花精油。本发明利用超临界CO2萃取经过处理的茉莉花浸膏，充分结合了溶剂浸提茉莉鲜花的低成本、处理量大的优势和超临界CO2萃取分离的高效率和无溶剂残留的优势，实现了溶剂残留量小，成本低，适于大规模生产茉莉花精油。A kind of extracting method of jasmine flower essential oil, to the jasmine flower extract obtained by leaching with sherwood oil or n-pentane, remove plant wax impurity by ethanol dissolution freezing, distill and recover solvent ethanol, water eluting alcohol makes crude jasmine essential oil, The crude jasmine essential oil is further separated with supercritical CO to remove the residual solvent, and the jasmine essential oil with pure fragrance is obtained. The present invention utilizes supercritical CO2 to extract the treated jasmine extract, fully combines the advantages of low cost and large processing capacity of solvent extraction of jasmine flowers and the advantages of high efficiency and no solvent residue in supercritical CO2 extraction and separation, and realizes The method has the advantages of small solvent residue and low cost, and is suitable for large-scale production of jasmine essential oil.
Description
技术领域technical field
本发明涉及一种提取天然香精香料技术领域，具体是一种茉莉花精油的提取方法。The invention relates to the technical field of extracting natural flavors and fragrances, in particular to a method for extracting jasmine essential oil.
背景技术Background technique
茉莉精油被称为“精油之王”，广泛用于各类香精尤其是顶级香水和顶级化妆品香精配方中及日用化妆品、医药、食品饮料、烟草、化工等产业，并具有生物激素功能，具有催情、调理生殖系统、促进乳汁分泌、调理干燥及敏感肌肤、淡化妊娠纹与疤痕、增加皮肤弹性等作用。有关超临界CO2提取茉莉花精油的研究，国内已有一些公开文献报道。如广西林业科学研究院与广西大学精细化工研究所对超临界CO2萃取桂花和茉莉花浸膏进行了研究，考察萃取时间、温度、压力对浸膏得率和质量的影响。茉莉花萃取最佳工艺条件为：压力12-15MPa，温度308-323K，时间1-1.5h，浸膏得率为0.240％。中国专利申请CN02152166.2公开了一种生产纯天然茉莉花精油的方法，该方法是在室温条件下，不经任何溶剂处理过程，用潮湿空气吹过分层放置的新鲜茉莉花，带出茉莉花散发的芳香成份，并用特殊吸附剂捕集，直至茉莉花吐香完毕，然后用超临界二氧化碳流体萃取回收吸附剂中的精油。中国专利申请CN201110374737.6公开了一种制备植物精油的方法，首先取原料，粉碎，置于萃取釜中，以超临界CO2流体为萃取溶剂，以体积浓度为55-65％的乙醇为夹带剂进行超临界萃取，经分离釜分离得到浸膏，然后将萃取所得的浸膏置于分子蒸馏器中进行分子蒸馏，收集得到相应的植物精油。中国专利申请CN200510018586.5公开了一种茉莉花精油的提取方法，先将茉莉鲜花在浸提机内逆流泳浸萃取，反复循环，萃取时间经1-3小时后，浸出液从浸提机流出，减压浓缩回收溶剂，使浸提液变粘稠放出冷却制成茉莉浸膏，然后将茉莉浸膏超临界CO2流体混合萃取，分离出的粗油经精馏柱分馏出水和残留溶剂及杂质后得到茉莉精油，采用该发明提取方法净油的得率可以达到48-55％。Jasmine essential oil is known as the "king of essential oils". It is widely used in various flavors, especially top-level perfumes and top-level cosmetic flavor formulas, as well as in daily cosmetics, medicine, food and beverage, tobacco, and chemical industries. It also has the function of biological hormones. Aphrodisiac, regulate reproductive system, promote milk secretion, regulate dry and sensitive skin, dilute stretch marks and scars, increase skin elasticity, etc. There have been some public literature reports on the research on supercritical CO2 extraction of jasmine essential oil. For example, the Guangxi Academy of Forestry Sciences and the Institute of Fine Chemical Engineering of Guangxi University have conducted research on the extraction of sweet-scented osmanthus and jasmine extracts with supercritical CO 2 , investigating the effects of extraction time, temperature, and pressure on the yield and quality of the extracts. The optimum technological conditions for Jasmine flower extraction are: pressure 12-15MPa, temperature 308-323K, time 1-1.5h, extract yield 0.240%. Chinese patent application CN02152166.2 discloses a method of producing pure natural jasmine essential oil. The method is to blow through fresh jasmine flowers layered with moist air at room temperature without any solvent treatment process to bring out the jasmine flower. Aromatic components are captured by a special adsorbent until the jasmine flower is exhaled, and then the essential oil in the adsorbent is recovered by supercritical carbon dioxide fluid extraction. Chinese patent application CN201110374737.6 discloses a method for preparing plant essential oils. First, the raw materials are taken, pulverized, placed in an extraction kettle, and supercritical CO2 fluid is used as the extraction solvent, and ethanol with a volume concentration of 55-65% is used as entrainment Extraction is carried out by supercritical extraction, and the extract is obtained by separation in a separation tank, and then the extracted extract is placed in a molecular still for molecular distillation, and the corresponding plant essential oil is collected. Chinese patent application CN200510018586.5 discloses a method for extracting jasmine essential oil. First, jasmine flowers are soaked and extracted by countercurrent swimming in the extraction machine, and the cycle is repeated. After the extraction time is 1-3 hours, the leachate flows out from the extraction machine, reducing Concentrate under pressure to recover the solvent, make the extract thicken, release it and cool it to make jasmine extract, then mix and extract the jasmine extract with supercritical CO2 fluid, and the separated crude oil is fractionated to remove water, residual solvent and impurities through the rectification column To obtain jasmine essential oil, the yield of absolute oil can reach 48-55% by adopting the extraction method of the invention.
现有茉莉花精油提取的技术中，多采有机溶剂浸提或者超临界CO2萃取茉莉鲜花制得茉莉浸膏，茉莉浸膏进一步提纯得茉莉精油(精油)。采用石油醚等有机溶剂浸提茉莉鲜花，容易造成茉莉花精油中有毒溶剂的残留；采用超临界CO2萃取茉莉鲜花，设备需要在高压条件下操作，规模上不去，生产成本高。也有利用活性炭等吸附剂吸附茉莉花香气，然后再用超临界CO2萃取回收活性炭中的精油，虽避免了有机溶剂污染，但是此法效率低，吸附剂再生困难，生产周期长。现有茉莉花精油生产技术的缺点主要在于有机溶剂的残留和超临界CO2萃取生产成本高这两个方面。In the existing jasmine essential oil extraction technology, organic solvent extraction or supercritical CO2 extraction of jasmine flowers is often used to obtain jasmine extract, and the jasmine extract is further purified to obtain jasmine essential oil (essential oil). Using organic solvents such as petroleum ether to extract jasmine flowers may easily cause the residue of toxic solvents in jasmine flower essential oil; using supercritical CO2 to extract jasmine flowers requires equipment to be operated under high pressure conditions, the scale cannot be increased, and the production cost is high. There are also adsorbents such as activated carbon to absorb the aroma of jasmine, and then use supercritical CO to extract and recover the essential oil in the activated carbon. Although organic solvent pollution is avoided, this method has low efficiency, difficult regeneration of adsorbent, and long production cycle. The disadvantages of the existing jasmine essential oil production technology mainly lie in the residue of organic solvent and the high production cost of supercritical CO2 extraction.
发明内容Contents of the invention
本发明的目的是提供一种溶剂残留量少，节能环保，成本低，适于规模化生产的茉莉花精油的提取方法。The purpose of the present invention is to provide a method for extracting jasmine essential oil with less solvent residue, energy saving, environmental protection, low cost and suitable for large-scale production.
为了实现上述目的，本发明的技术方案是：一种茉莉花精油的提取方法，包括如下步骤：In order to achieve the above object, the technical solution of the present invention is: a kind of extracting method of jasmine essential oil, comprises the steps:
a)将茉莉花浸膏和含量80-95％的食用乙醇按质量比为1:3-1:10一起加入反应釜，控制温度在50-70℃，搅拌0.5-1.0h，冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液；a) Add jasmine extract and edible ethanol with a content of 80-95% to the reaction kettle at a mass ratio of 1:3-1:10, control the temperature at 50-70°C, stir for 0.5-1.0h, and cool to 15-25 ℃, filter and remove the filter residue to obtain the ethanol extract of jasmine extract;
b)将得到的茉莉花浸膏的乙醇提取液先常压蒸馏0.5h，然后在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇，得到浓缩物；b) distill the ethanol extract of the obtained jasmine extract for 0.5 h at atmospheric pressure, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, reclaim the solvent ethanol, and obtain a concentrate;
c)取上述浓缩物，用水洗进一步脱除乙醇制得粗茉莉精油；c) take the above concentrate, wash with water to further remove ethanol to obtain crude jasmine essential oil;
d)取上述粗茉莉精油，在压力为8-10MPa，温度30-45℃条件下，用超临界CO2萃取1-2h。d) Take the above-mentioned crude jasmine essential oil, and extract it with supercritical CO 2 for 1-2 hours under the conditions of a pressure of 8-10 MPa and a temperature of 30-45°C.
e)采取降压法，解吸出溶解在临界CO2中的粗茉莉精油；E) adopt step-down method, desorb and go out and dissolve in critical CO The crude jasmine essential oil in the middle ;
f)重复a)-f)步骤，可以制得高品质茉莉花精油。f) repeat a)-f) steps, can make high-quality jasmine essential oil.
所述食用乙醇为含有0.1-0.3％的柠檬酸。The edible ethanol contains 0.1-0.3% citric acid.
所述食用乙醇为含有0.2-0.5％的CaCl2。The edible ethanol contains 0.2-0.5% CaCl 2 .
步骤d)所述超临界CO2萃取含有占CO2质量2-3％的H2O作为夹带剂。The supercritical CO 2 extraction in step d) contains H 2 O accounting for 2-3% by mass of CO 2 as an entrainer.
本发明的技术原理：Technical principle of the present invention:
采用石油醚、正戊烷、石油醚等有机溶剂浸提茉莉鲜花，经浓缩浸提液得到的茉莉花浸膏，往往含有残留的有机溶剂和超过50％的植物蜡等杂质。可以通过醇提的方法除去茉莉花浸膏的大部分杂质。本发明采用80-95％的食用乙醇，作为茉莉浸膏的溶剂，采用先溶解后冷冻的方法除去植物蜡等杂质。为了更好的将植物蜡等杂质除去，可以在上述食用乙醇中加入0.1％-0.3％的柠檬酸或者0.2％-0.5％的CaCl2。Adopt organic solvents such as sherwood oil, n-pentane, sherwood oil to leach jasmine flower, the jasmine flower extract that obtains through concentrating leaching solution often contains impurity such as residual organic solvent and more than 50% vegetable wax. Most of the impurities in jasmine extract can be removed by alcohol extraction. The invention adopts 80-95% edible ethanol as a solvent of jasmine extract, and adopts a method of dissolving and then freezing to remove impurities such as plant wax. In order to better remove impurities such as vegetable wax, 0.1%-0.3% citric acid or 0.2%-0.5% CaCl 2 may be added to the edible ethanol.
上述醇提后得到的滤液，通过先常压下蒸馏回收60-80％的溶剂，然后减压蒸馏进一步回收溶剂，这样可以减少溶剂挥发损失。但由于乙醇沸点较高而且其分子含有极性的羟基和非极性的烷基，当蒸馏浓缩物中乙醇含量降到一定程度，进一步蒸馏除去乙醇将造成茉莉花精油的香气成分的大量损失，而且由于乙醇与精油中的醇类、酯类等香气成分形成共沸，也较难除尽乙醇。为了避免蒸馏时间过长以及共沸现象造成的茉莉花精油成分的损失，所得浓缩物中乙醇残留量≤5％时，可以通过水来萃取茉莉花精油中的乙醇，来进一步脱除乙醇。用2-3倍体积的水与上述浓缩物混合搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。水洗后的粗茉莉精油乙醇含量≤1％，烃类有机溶剂含量≤0.5％。For the filtrate obtained after the alcohol extraction, 60-80% of the solvent is recovered by distillation under normal pressure, and then the solvent is further recovered by distillation under reduced pressure, so that the solvent volatilization loss can be reduced. But because ethanol boiling point is higher and its molecule contains polar hydroxyl group and nonpolar alkyl group, when ethanol content drops to a certain degree in the distillation concentrate, further distillation removes ethanol and will cause a large amount of loss of the fragrance component of jasmine flower essential oil, and Since ethanol forms an azeotrope with aroma components such as alcohols and esters in essential oils, it is also difficult to remove ethanol. In order to avoid the loss of jasmine essential oil components caused by excessive distillation time and azeotropic phenomenon, when the ethanol residue in the obtained concentrate is less than or equal to 5%, the ethanol in the jasmine essential oil can be extracted by water to further remove ethanol. Mix and stir 2-3 times the volume of water with the above-mentioned concentrate for 0.5-1h, statically separate layers, drain the lower layer of water, repeat washing with water 2-3 times, and the obtained concentrate is crude jasmine essential oil. The washed crude jasmine essential oil has an ethanol content of ≤1 percent and a hydrocarbon organic solvent content of ≤0.5 percent.
为了进一步除去粗茉莉精油中残留的溶剂等杂质，得到一级茉莉精油，可将上述粗茉莉精油，用超临界CO2萃取分离提纯。超临界萃取提纯的条件为：压力8-10MPa，温度30-45℃，时间1.5-2.0h。萃取后，采用减压的方法，从萃取剂CO2中分离出茉莉花精油。所得茉莉精油烃类有机溶剂≤10ppm。In order to further remove impurities such as solvents remaining in the crude jasmine essential oil to obtain first-grade jasmine essential oil, the above-mentioned crude jasmine essential oil can be extracted, separated and purified with supercritical CO 2 . The conditions for supercritical extraction and purification are: pressure 8-10MPa, temperature 30-45°C, time 1.5-2.0h. After extraction, adopt the method for decompression, from extractant CO , separate Jasmine essential oil. The obtained jasmine essential oil hydrocarbon organic solvent≤10ppm.
所述超临界CO2萃取可以采取使用夹带剂的方法，选取占CO2质量2-3％的H2O作为夹带剂，所提取的茉莉花精油香气更加纯正。The supercritical CO 2 extraction can adopt the method of using an entrainer, and H 2 O accounting for 2-3% of the CO 2 mass is selected as the entrainer, and the extracted jasmine essential oil has a purer aroma.
本发明的突出优点在于：The outstanding advantages of the present invention are:
利用超临界CO2萃取经过处理的茉莉花浸膏，充分结合了溶剂浸提茉莉鲜花的低成本、处理量大的优势和超临界CO2萃取分离的高效率和无溶剂残留的优势，实现了溶剂残留量小，成本低，适于大规模生产茉莉花精油。特别是在除去粗茉莉精油中乙醇过程中，在乙醇含量较低而不易蒸馏出时，通过水来萃取出精油中的乙醇，节省了能源，降低了原料损耗。Using supercritical CO2 to extract the treated jasmine extract, fully combining the advantages of low cost and large processing capacity of solvent extraction of jasmine flowers and the advantages of high efficiency and no solvent residue in supercritical CO2 extraction and separation, the solvent The residual amount is small, the cost is low, and it is suitable for large-scale production of jasmine essential oil. Especially in the process of removing ethanol in the crude jasmine essential oil, when the ethanol content is low and difficult to distill, the ethanol in the essential oil is extracted by water, which saves energy and reduces raw material loss.
具体实施方式Detailed ways
以下通过实施例对本发明的技术方案作进一步说明。本发明包括但不仅限于以下实施例。The technical solution of the present invention will be further described below through examples. The present invention includes but not limited to the following examples.
实施例1Example 1
取用石油醚提取的茉莉花浸膏1.0kg，与3.0kg含量为95％的食用乙醇一起加入反应釜。搅拌并加热，反应釜内温度控制在50-70℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇2.6kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.42kg，乙醇含量0.8％，烃类有机溶剂含量0.5％。将粗茉莉精油在压力为8-10MPa，温度30-45℃条件下，用超临界CO2萃取1.5-2.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.39kg，颜色浅黄，具有浓郁的茉莉花香气，其密度为0.956，折光指数1.4865，酸值25，烃类有机溶剂含量8ppm。Take 1.0 kg of jasmine extract extracted with petroleum ether, and add 3.0 kg of 95% edible ethanol into the reactor. Stir and heat, the temperature in the reactor is controlled at 50-70°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at vacuum degree -0.09 MPa for 0.5-1.0 h, and recover 2.6 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.42 kg, an ethanol content of 0.8%, and a hydrocarbon organic solvent content of 0.5%. The crude jasmine essential oil is extracted with supercritical CO 2 for 1.5-2.0 h at a pressure of 8-10 MPa and a temperature of 30-45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.39kg, is light yellow in color, has strong jasmine fragrance, has a density of 0.956, a refractive index of 1.4865, an acid value of 25, and a hydrocarbon organic solvent content of 8ppm.
实施例2Example 2
取用石油醚提取的茉莉花浸膏1.0kg，与5.0kg含量为85％的食用乙醇一起加入反应釜。搅拌并加热，反应釜内温度控制在50-70℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.5kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.45kg，乙醇含量0.9％，烃类有机溶剂含量0.3％。将粗茉莉精油在压力为10MPa，温度45℃条件下，用超临界CO2萃取1.5h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.43kg，颜色浅黄，具有浓郁的茉莉花香气，其密度为0.915，折光指数1.48605，酸值24，烃类有机溶剂含量10ppm。Take 1.0 kg of jasmine extract extracted with petroleum ether, and add 5.0 kg of edible ethanol with a content of 85% into the reactor. Stir and heat, the temperature in the reactor is controlled at 50-70°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at vacuum degree -0.09 MPa for 0.5-1.0 h, and recover 4.5 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.45 kg, an ethanol content of 0.9%, and a hydrocarbon organic solvent content of 0.3%. The crude jasmine essential oil was extracted with supercritical CO 2 for 1.5 h at a pressure of 10 MPa and a temperature of 45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.43kg, is light yellow in color, has strong jasmine aroma, has a density of 0.915, a refractive index of 1.48605, an acid value of 24, and a hydrocarbon organic solvent content of 10 ppm.
实施例3Example 3
取用正戊烷提取的茉莉花浸膏1.0kg，与10.0kg含量为80％的食用乙醇一起加入反应釜。搅拌并加热，反应釜内温度控制在50-70℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇7.8kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.47kg，乙醇含量1％，烃类有机溶剂含量0.5％。将粗茉莉精油在压力为8-10MPa，温度30-45℃条件下，用超临界CO2萃取1.5-2.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.42kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.924，折光指数1.4875，酸值22，烃类有机溶剂含量9ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, and add 10.0 kg of 80% edible ethanol into the reactor. Stir and heat, the temperature in the reactor is controlled at 50-70°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at vacuum degree -0.09 MPa for 0.5-1.0 h, and recover 7.8 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.47 kg, an ethanol content of 1%, and a hydrocarbon organic solvent content of 0.5%. The crude jasmine essential oil is extracted with supercritical CO 2 for 1.5-2.0 h at a pressure of 8-10 MPa and a temperature of 30-45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.42kg, is light yellow in color, has strong jasmine aroma, has a density of 0.924, a refractive index of 1.4875, an acid value of 22, and a hydrocarbon organic solvent content of 9ppm.
实施例4Example 4
取用正戊烷提取的茉莉花浸膏1.0kg，与6.0kg含量为85％的食用乙醇以及6g柠檬酸一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.8kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.45kg，乙醇含量0.7％，烃类有机溶剂含量0.5％。将粗茉莉精油在压力为9MPa，温度45℃条件下，用超临界CO2萃取2.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.40kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.976，折光指数1.4890，酸值20，烃类有机溶剂含量7ppm。Take 1.0 kg of jasmine flower extract extracted with n-pentane, add 6.0 kg of 85% edible ethanol and 6 g of citric acid into the reaction kettle. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at vacuum degree -0.09 MPa for 0.5-1.0 h, and recover 4.8 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.45 kg, an ethanol content of 0.7%, and a hydrocarbon organic solvent content of 0.5%. The crude jasmine essential oil was extracted with supercritical CO 2 for 2.0 hours at a pressure of 9 MPa and a temperature of 45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil is 0.40kg, light yellow in color, has a strong jasmine fragrance, its density is 0.976, its refractive index is 1.4890, its acid value is 20, and its hydrocarbon organic solvent content is 7ppm.
实施例5Example 5
取用正戊烷提取的茉莉花浸膏1.0kg，与3.5kg含量为95％的食用乙醇以及10g柠檬酸一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇2.8kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.45kg，乙醇含量0.8％，烃类有机溶剂含量0.5％。将粗茉莉精油在压力为8MPa，温度30℃条件下，用超临界CO2萃取1.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.42kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.956，折光指数1.4885，酸值23，烃类有机溶剂含量8ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, and add 3.5 kg of 95% edible ethanol and 10 g of citric acid into the reaction kettle. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at vacuum degree -0.09 MPa for 0.5-1.0 h, and recover 2.8 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.45 kg, an ethanol content of 0.8%, and a hydrocarbon organic solvent content of 0.5%. The crude jasmine essential oil was extracted with supercritical CO 2 for 1.0 h at a pressure of 8 MPa and a temperature of 30°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.42kg, is light yellow in color, has strong jasmine aroma, has a density of 0.956, a refractive index of 1.4885, an acid value of 23, and a hydrocarbon organic solvent content of 8ppm.
实施例6Example 6
取用正戊烷提取的茉莉花浸膏1.0kg，与9.0kg含量为85％的食用乙醇以及15g柠檬酸一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏1.0h，回收溶剂乙醇7.8kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.41kg，乙醇含量1％，烃类有机溶剂含量0.3％。将粗茉莉精油在压力为9MPa，温度30-45℃条件下，用超临界CO2萃取1.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.43kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.956，折光指数1.4885，酸值27，烃类有机溶剂含量10ppm。Take 1.0 kg of jasmine flower extract extracted with n-pentane, and add 9.0 kg of edible ethanol with a content of 85% and 15 g of citric acid into the reaction kettle. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. The above-mentioned extract was distilled at atmospheric pressure for 0.5 h, and then distilled under reduced pressure at a vacuum degree of -0.09 MPa for 1.0 h to recover 7.8 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.41 kg, an ethanol content of 1%, and a hydrocarbon organic solvent content of 0.3%. The crude jasmine essential oil was extracted with supercritical CO 2 for 1.0 h at a pressure of 9 MPa and a temperature of 30-45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.43kg, is light yellow in color, has strong jasmine fragrance, has a density of 0.956, a refractive index of 1.4885, an acid value of 27, and a hydrocarbon organic solvent content of 10ppm.
实施例7Example 7
取用石油醚提取的茉莉花浸膏1.0kg，与5.0kg含量为85％的食用乙醇以及10gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.47kg，乙醇含量0.85％，烃类有机溶剂含量0.45％。将粗茉莉精油在压力为8.5MPa，温度39℃条件下，用超临界CO2萃取1.5h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.42kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.976，折光指数1.4885，酸值20，烃类有机溶剂含量10ppm。Take 1.0 kg of jasmine extract extracted with petroleum ether, 5.0 kg of 85% edible ethanol and 10 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.47kg, an ethanol content of 0.85%, and a hydrocarbon organic solvent content of 0.45%. The crude jasmine essential oil was extracted with supercritical CO 2 for 1.5 h at a pressure of 8.5 MPa and a temperature of 39 °C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.42kg, is light yellow in color, has strong jasmine aroma, has a density of 0.976, a refractive index of 1.4885, an acid value of 20, and a hydrocarbon organic solvent content of 10ppm.
实施例8Example 8
取用石油醚提取的茉莉花浸膏1.0kg，与5.0kg含量为85％的食用乙醇以及25gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.43kg，乙醇含量0.8％，烃类有机溶剂含量0.5％。将粗茉莉精油在压力为9MPa，温度35℃条件下，用超临界CO2萃取1.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.39kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.934，折光指数1.4875，酸值15，烃类有机溶剂含量8ppm。Take 1.0 kg of jasmine extract extracted with petroleum ether, 5.0 kg of 85% edible ethanol and 25 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.43 kg, an ethanol content of 0.8%, and a hydrocarbon organic solvent content of 0.5%. The crude jasmine essential oil was extracted with supercritical CO 2 for 1.0 h at a pressure of 9 MPa and a temperature of 35°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.39kg, is light yellow in color, has strong jasmine aroma, has a density of 0.934, a refractive index of 1.4875, an acid value of 15, and a hydrocarbon organic solvent content of 8ppm.
实施例9Example 9
取用正戊烷提取的茉莉花浸膏1.0kg，与5.0kg含量为85％的食用乙醇以及15gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.51kg，乙醇含量1％，烃类有机溶剂含量0.45％。将粗茉莉精油在压力为10MPa，温度45℃条件下，用超临界CO2萃取2.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.45kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.966，折光指数1.4893，酸值18，烃类有机溶剂含量9ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, 5.0 kg of 85% edible ethanol and 15 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.51 kg, an ethanol content of 1%, and a hydrocarbon organic solvent content of 0.45%. The crude jasmine essential oil was extracted with supercritical CO 2 for 2.0 hours at a pressure of 10 MPa and a temperature of 45°C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.45kg, is light yellow in color, has strong jasmine aroma, has a density of 0.966, a refractive index of 1.4893, an acid value of 18, and a hydrocarbon organic solvent content of 9ppm.
实施例10Example 10
取用正戊烷提取的茉莉花浸膏1.0kg，与6.0kg含量为85％的食用乙醇以及15gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.49kg，乙醇含量0.7％，烃类有机溶剂含量0.3％。用超临界CO2和占CO2质量3％的H2O作为夹带剂，将粗茉莉精油在压力为10MPa，温度37℃条件下，用超临界CO2萃取1.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.45kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.975，折光指数1.4876，酸值19，烃类有机溶剂含量7ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, 6.0 kg of 85% edible ethanol and 15 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.49 kg, an ethanol content of 0.7%, and a hydrocarbon organic solvent content of 0.3%. Using supercritical CO 2 and H 2 O accounting for 3% of the mass of CO 2 as entrainers, the crude jasmine essential oil was extracted with supercritical CO 2 for 1.0 h at a pressure of 10 MPa and a temperature of 37° C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.45kg, is light yellow in color, has strong jasmine aroma, has a density of 0.975, a refractive index of 1.4876, an acid value of 19, and a hydrocarbon organic solvent content of 7ppm.
实施例11Example 11
取用正戊烷提取的茉莉花浸膏1.0kg，与6.0kg含量为85％的食用乙醇以及15gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.49kg，乙醇含量0.9％，烃类有机溶剂含量0.4％。用超临界CO2和占CO2质量2.5％的H2O作为夹带剂，将粗茉莉精油在压力为9.7MPa，温度42℃条件下，用超临界CO2萃取1.5h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.42kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.938，折光指数1.4895，酸值25，烃类有机溶剂含量5ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, 6.0 kg of 85% edible ethanol and 15 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.49 kg, an ethanol content of 0.9%, and a hydrocarbon organic solvent content of 0.4%. Using supercritical CO 2 and H 2 O accounting for 2.5% of the mass of CO 2 as entraining agents, the crude jasmine essential oil was extracted with supercritical CO 2 for 1.5 h at a pressure of 9.7 MPa and a temperature of 42° C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.42kg, is light yellow in color, has strong jasmine fragrance, has a density of 0.938, a refractive index of 1.4895, an acid value of 25, and a hydrocarbon organic solvent content of 5ppm.
实施例12Example 12
取用正戊烷提取的茉莉花浸膏1.0kg，与6.0kg含量为85％的食用乙醇以及15gCaCl2。一起加入反应釜。搅拌并加热，反应釜内温度控制在50-60℃，搅拌时间0.5-1.0h。停止加热和搅拌，通冷凝水，将反应釜内原料冷却至15-25℃，过滤除去滤渣，得到茉莉花浸膏的乙醇提取液。将上述提取液先常压蒸馏0.5h，在真空度-0.09MPa减压蒸馏0.5-1.0h，回收溶剂乙醇4.2kg。所得浓缩物用2-3倍体积的水混合，搅拌0.5-1h，静止分层，排出下层水，重复水洗2-3遍，所得浓缩物即为粗茉莉精油。所得粗茉莉精油，质量0.42kg，乙醇含量0.75％，烃类有机溶剂含量0.37％。用超临界CO2和占CO2质量2％的H2O作为夹带剂，将粗茉莉精油在压力为9.5MPa，温度42℃条件下，用超临界CO2萃取2.0h。萃取结束后，降低压力到3MPa，从萃取剂CO2中分离出茉莉花精油。萃取剂CO2加压后继续使用。所得茉莉精油为0.43kg，颜色浅黄，具有浓郁的茉莉花香气，其密度0.926，折光指数1.4882，酸值21，烃类有机溶剂含量6ppm。Take 1.0 kg of jasmine extract extracted with n-pentane, 6.0 kg of 85% edible ethanol and 15 g of CaCl 2 . Add to the reactor together. Stir and heat, the temperature in the reactor is controlled at 50-60°C, and the stirring time is 0.5-1.0h. Stop heating and stirring, pass condensed water, cool the raw materials in the reaction kettle to 15-25°C, filter and remove the filter residue, and obtain the ethanol extract of jasmine flower extract. Distill the above extract under normal pressure for 0.5 h, then distill under reduced pressure at a vacuum degree of -0.09 MPa for 0.5-1.0 h, and recover 4.2 kg of solvent ethanol. The obtained concentrate is mixed with 2-3 times the volume of water, stirred for 0.5-1h, statically separated into layers, the lower layer of water is drained, and washed with water for 2-3 times repeatedly, and the obtained concentrate is crude jasmine essential oil. The obtained crude jasmine essential oil has a mass of 0.42 kg, an ethanol content of 0.75%, and a hydrocarbon organic solvent content of 0.37%. Using supercritical CO 2 and H 2 O accounting for 2% of the mass of CO 2 as entraining agents, the crude jasmine essential oil was extracted with supercritical CO 2 for 2.0 h at a pressure of 9.5 MPa and a temperature of 42° C. After extraction finishes, reduce pressure to 3MPa, from extraction agent CO Separate out jasmine essential oil. The extractant CO2 is pressurized and then used. The obtained jasmine essential oil weighs 0.43kg, is light yellow in color, has strong jasmine aroma, has a density of 0.926, a refractive index of 1.4882, an acid value of 21, and a hydrocarbon organic solvent content of 6ppm.
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